CN102778486A - Potential measurement method of cold-rolled enameling sheet steel sensitivity - Google Patents
Potential measurement method of cold-rolled enameling sheet steel sensitivity Download PDFInfo
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- CN102778486A CN102778486A CN2012102891251A CN201210289125A CN102778486A CN 102778486 A CN102778486 A CN 102778486A CN 2012102891251 A CN2012102891251 A CN 2012102891251A CN 201210289125 A CN201210289125 A CN 201210289125A CN 102778486 A CN102778486 A CN 102778486A
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Abstract
The invention discloses a potential measurement method of cold-rolled enameling sheet steel sensitivity. The potential measurement method comprises the following steps: cleaning a sample; fastening the sample between two electrolytic cells; controlling the test temperature to be 25+/-0.5 DEG C; introducing electrolyte in the two electrolytic cells simultaneously; measuring a potential value of the sample, and after the potential value of the sample is stabilized, charging hydrogen into the sample; recording a potential-time curve of the sample by a computer, and when the potential-time curve is a straight line approximately parallel to horizontal ordinates, stopping the test; and obtaining hydrogen permeation time through the potential-time curve, and calculating an enameling fish-scaling resistance sensitive value according to the hydrogen permeation time. The measurement method provided by the invention is simple in operation, short in test period and high in working efficiency.
Description
Technical field
The present invention relates to detect the field of cold-rolled steel sheet performance, be meant a kind of potential measurement method of cold-rolled steel sheet enamel susceptibility especially.
Background technology
Be dissolved into the hydrogen in the steel plate with atomic form in the enamel firing manufacturing process; Between the hole of enamel coating and metal interface or enamel coating and metal interface, combine bad zone to form molecular hydrogen; The interfacial pressure that these hydrogen form reaches the critical value of destroying enamel coating; Broken in the enamel surface, it is quick-fried that this phenomenon is called squama.Squama is quick-fried to be the modal defective that influences the enamel product quality, for the correct quick-fried cold-reduced sheet of anti-squama of selecting, reduces the quick-fried loss of squama of enamel product, need test the quick-fried performance of the anti-enamel squama of cold-rolled steel sheet.The quick-fried susceptibility of cold-rolled steel sheet enamel squama just is meant the possibility of breaking at the cold-rolled steel sheet enameling, and what its essence reflected is the transmissibility of atomic hydrogen in the cold-rolled steel sheet.For enamelled pressed steel; When hydrogen spreads slowly more in enamelled pressed steel, the time that promptly penetrates steel plate is long more, and the quick-fried performance of anti-enamel squama of steel plate is just good more; Usually people adopt the hydrogen time of penetration to weigh the diffusion speed of hydrogen in metal, thereby estimate the quick-fried performance of enamel squama of cold-rolled steel sheet.
Application number is that 201110103016.1 Chinese patent discloses the quick-fried service check method of the anti-enamel squama of a kind of cold-rolled steel sheet, and its principle is electrolysis when filling hydrogen, H
+Arrival is reduced into H and gets into sample as the specimen surface of negative electrode, diffuses to the another side of sample, and H is become H by electrolytic oxidation again
+,, assess the diffusion process of H in sample through detecting the anode current of H oxidizing process.The required time be called the hydrogen time of penetration when hydrogen diffusion reaches when stablize, the hydrogen time of penetration is long more, and the quick-fried performance of anti-enamel squama is just good more.
Above-mentioned detection method is specially: at first in expanding the hydrogen electrolytic tank, pour sodium hydroxide solution into and add constant potential 0.3V for the sample end that expands in the hydrogen electrolytic tank through potentiostat, to remove hydrogen original in the sample; Then, the electric current of the sample end in expanding the hydrogen electrolytic tank is reduced to below the 1.5 μ A, in filling the hydrogen electrolytic tank, pours the mixed solution of sulfuric acid and thiocarbamide into, and the demand working galvanostat, keeps 1.0mA/cm
2Current density sample is filled hydrogen.Then, along with the carrying out of filling the hydrogen process, can obtain on the computing machine to expand that anode current is the electric current of sample and the curve of time relationship in the hydrogen electrolytic tank; After after a while; It is stable that anode current keeps, and when one section platform appears in anode current～time curve, stops test.At last, mathematics manipulation and analysis through antianode electric current～time curve can obtain the hydrogen time of penetration, the hydrogen time of penetration are updated to the value that can calculate the quick-fried susceptibility of the anti-enamel squama of cold-rolled steel sheet in the computing formula of the quick-fried susceptibility of the anti-enamel squama of cold-rolled steel sheet.
Yet, in said method, on the one hand; Owing to before filling hydrogen on-test, must add constant potential, remove steel plate production earlier and deposit the hydrogen that absorbs in the process, and this process consumed time be very long at anode tap; Thereby causing the test period longer, efficient is not high.On the other hand, the equipment that the process of the hydrogen that electrolysis is come from the diffusion of expansion hydrogen electrolytic tank, is adopted is potentiostat, thereby makes that existing proving installation price is higher, and operation is comparatively complicated.
Summary of the invention
The object of the invention is exactly the potential measurement method that the quick-fried susceptibility of a kind of cold-rolled steel sheet enamel squama will be provided, and this method is simple to operate, the test period is short and high efficiency.
For realizing above-mentioned purpose, the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama that the present invention designed comprises the steps: 1) with the two-sided polishing of sand paper, clean with acetone and absolute ethyl alcohol successively again the cold-rolled steel sheet sample; 2) will fill the hydrogen electrolytic tank and expand the hydrogen electrolytic tank and contact also fasteningly respectively through O type sealing ring with the two sides of sample, the diameter of the surface of contact of sample and two electrolytic tanks is 10 ~ 15mm; 3) temperature with test is controlled at 25 ± 0.5 ℃; 4) in filling hydrogen electrolytic tank and expansion hydrogen electrolytic tank, add 0.1mol/LNaOH solution simultaneously, and make sample all immerse in the said solution, wherein; In filling the hydrogen electrolytic tank, sample is as negative electrode, and platinum filament or platinized platinum are as anode; In expanding the hydrogen electrolytic tank, be provided with contrast electrode; 5) measure to expand the potential value of sample in the hydrogen electrolytic tank, treat that the potential value of sample is stable after, in filling the hydrogen electrolytic tank, keep 1.5mA/cm
2Current density sample is filled hydrogen; 6) when filling hydrogen and begin, timing immediately, this moment is for filling hydrogen start time t
0, obtain to expand the potential value of sample in the hydrogen electrolytic tank and fill the curve of hydrogen time, i.e. current potential ~ time curve through computing machine simultaneously; Wherein, horizontal ordinate is for filling the hydrogen time, and ordinate is the potential value of sample; When current potential ~ time curve occur one section approximate when being parallel to the straight line of horizontal ordinate, stop test; 7) choose and fill hydrogen start time t
0Later current potential ~ time curve is a research object, crosses the straight-line segment of testing early stage on this current potential ~ time curve and makes a straight line, and cross the straight-line segment in test later stage on this current potential ~ time curve and make another straight line, and the horizontal ordinate of two straight-line intersections is hydrogen time of penetration t
b8) according to formula KB=t
b/ d
2Calculate the quick-fried sensitivity value of anti-enamel squama of sample, wherein, t
bBe the hydrogen time of penetration, d is the thickness of sample.
Further, in the said step 5), adopt potential difference meter to measure the potential value that expands sample in the hydrogen electrolytic tank.
Further, in the said step 5), adopt galvanostat to produce 1.5mA/cm
2Current density sample is filled hydrogen.
Test shows that the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of the present invention has following beneficial effect:
1, because the hydrogen that keeps in the sample before the test is little to the current potential influence of measuring sample; Thereby when adopting potential measurement method of the present invention that the quick-fried performance of the anti-enamel squama of cold-rolled steel sheet is detected; Need not sample is carried out pre-service, thereby shortened the test period, improved work efficiency;
What 2, the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of the present invention was measured is the potential value of sample, only needs contrast electrode and potential difference meter during measurement, thereby, but the not only step of simplified measurement and operation, and can reduce production costs;
3, because in 1 year, the environment temperature many places in about 25 ℃, thereby, the temperature of test is controlled at 25 ± 0.5 ℃, realize more easily;
4, expand the hydrogen electrolytic tank among the present invention and the testing liquid that fills in the hydrogen electrolytic tank is 0.1mol/L NaOH solution; Employing with a kind of testing liquid not only can simplify solution preparation, reduce the test vessel take, practiced thrift chemical reagent; And simplified operation, the contingent problem that adds wrong solution in liquid and the test of scurrying when fundamentally having avoided between two electrolytic tanks, loading and unloading sample, simultaneously; Also reduced the discharging of waste liquid, more environmental protection;
5, fill area that the hydrogen current density depends on the kind of filling the hydrogen electrolytic tank and expanding the testing liquid in the hydrogen electrolytic tank, sample contact test solution, expand the hydrogen conductive quantity that the hydrogen detection technique that adopts in the hydrogen electrolytic tank and steel plate allow; And fill the length that the hydrogen current density has also determined test period; Be a very important parameter, when filling the hydrogen current density when excessive, though can shorten test period; But might cause that sample bubbles the result that must make mistake; The hydrogen current density is less than normal when filling, and can prolong test period, simultaneously the hydrogen detection technique sensitivity of expanding in the hydrogen electrolytic tank is had very high requirement.The present invention selects 1.5mA/cm for use
2Current density to fill hydrogen be to select meticulously according to test condition, be complementary with this test condition.
Description of drawings
The structural representation of the measurement mechanism that Fig. 1 is adopted for the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of the present invention.
Fig. 2 is the current potential ~ time plot of the potential measurement method acquisition of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of the present invention.
Embodiment
Below in conjunction with specific embodiment the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of the present invention is done further to describe in detail.
Embodiment 1
With reference to Fig. 1 and 2, the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of present embodiment comprises the steps:
1) uses sand paper with the two-sided polishing of thickness d, clean with acetone and absolute ethyl alcohol successively again as the DC03 cold-rolled steel sheet sample 3 of 0.8mm;
2) will fill hydrogen electrolytic tank 1 and expand hydrogen electrolytic tank 2 and contact also fasteningly respectively through O type sealing ring with the two sides of sample 3, the diameter of the surface of contact of sample 3 and two electrolytic tanks 1,2 is 10mm;
3) temperature with test is controlled at 25 ± 0.5 ℃;
4) in filling hydrogen electrolytic tank 1 and expansion hydrogen electrolytic tank 2, add 0.1mol/L NaOH solution simultaneously, and make sample 3 all immerse in the said solution, wherein; In filling hydrogen electrolytic tank 1, sample 3 is as negative electrode, and platinum filament or platinized platinum 4 are as anode; In expanding hydrogen electrolytic tank 2, be provided with contrast electrode 5;
5) adopt potential difference meter 7 to measure the potential value that expands sample 3 in the hydrogen electrolytic tanks 2, treat that the potential value of sample 3 is stable after, in filling hydrogen electrolytic tank 1, demand working galvanostat 6 keeps 1.5mA/cm
2 Current density sample 3 is filled hydrogen;
6) when filling hydrogen and begin, timing immediately, this moment is for filling hydrogen start time t
0, obtaining to expand the potential value of sample 3 in the hydrogen electrolytic tank 2 and fill the curve of hydrogen time through computing machine 8 simultaneously is current potential ~ time curve, wherein; Horizontal ordinate is for filling the hydrogen time; Ordinate is the potential value of sample, when current potential ~ time curve occur one section approximate when being parallel to the straight line of horizontal ordinate, stop test;
7) choose and fill hydrogen start time t
0Later current potential ~ time curve is a research object; The test straight-line segment of crossing on this current potential ~ time curve C is in earlier stage made a straight line L1; And the straight-line segment of spending the test later stage on this current potential ~ time curve C makes another straight line L2, and the horizontal ordinate of the intersection point of two straight line L1, L2 is hydrogen time of penetration t
b
8) according to formula KB=t
b/ d
2Calculate the quick-fried sensitivity value of anti-enamel squama of sample, testing result reference table 1.For same type of cold-reduced sheet, the KB value is big more, shows that the quick-fried performance of its anti-enamel squama is good more.
The testing result of the DC03 cold-rolled steel sheet that table 1 Wuhan Iron and Steel Plant two cold rolling mills are produced
As can be seen from the above table, the mean value of KB is 24.2.Enamel is made test findings and is shown, 7 these steel grade samples have 1, and that squama has taken place is quick-fried, and the quick-fried incidence of squama is 14.3%, shows the quick-fried better performances of the anti-enamel squama of this cold-rolled steel sheet.
Embodiment 2
With reference to Fig. 1 and 2, the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of present embodiment comprises the steps:;
1) uses sand paper with the two-sided polishing of thickness d, clean with acetone and absolute ethyl alcohol successively again as the DC01 cold-rolled steel sheet sample 3 of 0.9mm;
2) will fill hydrogen electrolytic tank 1 and expand hydrogen electrolytic tank 2 and contact also fasteningly respectively through O type sealing ring with the two sides of sample 3, the diameter of the surface of contact of sample 3 and two electrolytic tanks 1,2 is 12mm;
3) temperature with test is controlled at 25 ± 0.5 ℃;
4) in filling hydrogen electrolytic tank 1 and expansion hydrogen electrolytic tank 2, add 0.1mol/L NaOH solution simultaneously, and make sample 3 all immerse in the said solution, wherein; In filling hydrogen electrolytic tank 1, sample 3 is as negative electrode, and platinum filament or platinized platinum 4 are as anode; In expanding hydrogen electrolytic tank 2, be provided with contrast electrode 5;
5) adopt potential difference meter 7 to measure the potential value that expands sample 3 in the hydrogen electrolytic tanks 2, treat that the potential value of sample 3 is stable after, in filling hydrogen electrolytic tank 1, demand working galvanostat 6 keeps 1.5mA/cm
2 Current density sample 3 is filled hydrogen;
6) when filling hydrogen and begin, timing immediately, this moment is for filling hydrogen start time t
0, obtaining to expand the potential value of sample 3 in the hydrogen electrolytic tank 2 and fill the curve of hydrogen time through computing machine 8 simultaneously is current potential ~ time curve, wherein; Horizontal ordinate is for filling the hydrogen time; Ordinate is the potential value of sample, when current potential ~ time curve occur one section approximate when being parallel to the straight line of horizontal ordinate, stop test;
7) choose and fill hydrogen start time t
0Later current potential ~ time curve is a research object; The test straight-line segment of crossing on this current potential ~ time curve C is in earlier stage made a straight line L1; And the straight-line segment of spending the test later stage on this current potential ~ time curve C makes another straight line L2, and the horizontal ordinate of the intersection point of two straight line L1, L2 is hydrogen time of penetration t
b
8) according to formula KB=t
b/ d
2Calculate the quick-fried sensitivity value of anti-enamel squama of sample, testing result reference table 2.For same type of cold-reduced sheet, the KB value is big more, shows that the quick-fried performance of its anti-enamel squama is good more.
The testing result of the DC01 cold-rolled steel sheet that table 2 Wuhan Iron and Steel Plant two cold rolling mills are produced
As can be seen from the above table, the mean value of KB is 26.9.Enamel is made test findings and is shown, it is quick-fried that squama does not take place all for 7 these steel grade samples, and the quick-fried incidence of squama is 0%, shows that the quick-fried performance of the anti-enamel squama of this cold-rolled steel sheet is fine.
With reference to Fig. 1 and 2, the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama of present embodiment comprises the steps:
1) uses sand paper with the two-sided polishing of thickness d, clean with acetone and absolute ethyl alcohol successively again as the DC03 cold-rolled steel sheet sample 3 of 1.0mm;
2) will fill hydrogen electrolytic tank 1 and expand hydrogen electrolytic tank 2 and contact also fasteningly respectively through O type sealing ring with the two sides of sample 3, the diameter of the surface of contact of sample 3 and two electrolytic tanks 1,2 is 15mm;
3) temperature with test is controlled at 25 ± 0.5 ℃;
4) in filling hydrogen electrolytic tank 1 and expansion hydrogen electrolytic tank 2, add 0.1mol/L NaOH solution simultaneously, and make sample 3 all immerse in the said solution, wherein; In filling hydrogen electrolytic tank 1, sample 3 is as negative electrode, and platinum filament or platinized platinum 4 are as anode; In expanding hydrogen electrolytic tank 2, be provided with contrast electrode 5;
5) adopt potential difference meter 7 to measure the potential value that expands sample 3 in the hydrogen electrolytic tanks 2, treat that the potential value of sample 3 is stable after, in filling hydrogen electrolytic tank 1, demand working galvanostat 6 keeps 1.5mA/cm
2 Current density sample 3 is filled hydrogen;
6) when filling hydrogen and begin, timing immediately, this moment is for filling hydrogen start time t
0, obtaining to expand the potential value of sample 3 in the hydrogen electrolytic tank 2 and fill the curve of hydrogen time through computing machine 8 simultaneously is current potential ~ time curve, wherein; Horizontal ordinate is for filling the hydrogen time; Ordinate is the potential value of sample, when current potential ~ time curve occur one section approximate when being parallel to the straight line of horizontal ordinate, stop test;
7) choose and fill hydrogen start time t
0Later current potential ~ time curve is a research object; The test straight-line segment of crossing on this current potential ~ time curve C is in earlier stage made a straight line L1; And the straight-line segment of spending the test later stage on this current potential ~ time curve C makes another straight line L2, and the horizontal ordinate of the intersection point of two straight line L1, L2 is hydrogen time of penetration t
b
8) according to formula KB=t
b/ d
2Calculate the quick-fried sensitivity value of anti-enamel squama of sample, testing result reference table 3.For same type of cold-reduced sheet, the KB value is big more, shows that the quick-fried performance of its anti-enamel squama is good more.
The testing result of the DC03 cold-rolled steel sheet that table 3 Wuhan Iron and Steel Plant one cold rolling mill is produced
As can be seen from the above table, the mean value of KB is 22.5.Enamel is made test findings and is shown, it is quick-fried that squama has all taken place for 7 these steel grade samples, and the quick-fried incidence of squama is 100%, shows the quick-fried poor-performing of the anti-enamel squama of this cold-rolled steel sheet.
Claims (3)
1. the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama, it is characterized in that: this method comprises the steps:
1), cleans with acetone and absolute ethyl alcohol successively again with the two-sided polishing of sand paper with the cold-rolled steel sheet sample;
2) will fill the hydrogen electrolytic tank and expand the hydrogen electrolytic tank and contact also fasteningly respectively through O type sealing ring with the two sides of sample, the diameter of the surface of contact of sample and two electrolytic tanks is 10 ~ 15mm;
3) temperature with test is controlled at 25 ± 0.5 ℃;
4) in filling hydrogen electrolytic tank and expansion hydrogen electrolytic tank, add 0.1mol/L NaOH solution simultaneously, and make sample all immerse in the said solution, wherein; In filling the hydrogen electrolytic tank, sample is as negative electrode, and platinum filament or platinized platinum are as anode; In expanding the hydrogen electrolytic tank, be provided with contrast electrode;
5) measure to expand the potential value of sample in the hydrogen electrolytic tank, treat that the potential value of sample is stable after, in filling the hydrogen electrolytic tank, keep 1.5mA/cm
2Current density sample is filled hydrogen;
6) when filling hydrogen and begin, timing immediately, this moment is for filling hydrogen start time t
0, obtain to expand the potential value of sample in the hydrogen electrolytic tank and fill the curve of hydrogen time, i.e. current potential ~ time curve through computing machine simultaneously; Wherein, horizontal ordinate is for filling the hydrogen time, and ordinate is the potential value of sample; When current potential ~ time curve occur one section approximate when being parallel to the straight line of horizontal ordinate, stop test;
7) choose and fill hydrogen start time t
0Later current potential ~ time curve is a research object, crosses the straight-line segment of testing early stage on this current potential ~ time curve and makes a straight line, and cross the straight-line segment in test later stage on this current potential ~ time curve and make another straight line, and the horizontal ordinate of two straight-line intersections is hydrogen time of penetration t
b
8) according to formula KB=t
b/ d
2Calculate the quick-fried sensitivity value of anti-enamel squama of sample, wherein, t
bBe the hydrogen time of penetration, d is the thickness of sample.
2. the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama according to claim 1 is characterized in that: in the said step 5), adopt potential difference meter to measure the potential value that expands sample in the hydrogen electrolytic tank.
3. the potential measurement method of the quick-fried susceptibility of cold-rolled steel sheet enamel squama according to claim 1 and 2 is characterized in that: in the said step 5), adopt galvanostat to produce 1.5mA/cm
2Current density sample is filled hydrogen.
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Cited By (3)
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| CN107525908A (en) * | 2017-06-28 | 2017-12-29 | 柳州钢铁股份有限公司 | Water heater liner cold rolling glassed steel fish scaling resistance detection method |
| CN110095523A (en) * | 2018-01-29 | 2019-08-06 | 宝山钢铁股份有限公司 | A method of the prediction quick-fried occurrence probability size of enamelware squama |
| CN111693426A (en) * | 2019-03-15 | 2020-09-22 | 宝山钢铁股份有限公司 | Device and method for evaluating fish scaling performance of enamel steel |
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| CN107525908B (en) * | 2017-06-28 | 2020-07-28 | 柳州钢铁股份有限公司 | Method for detecting anti-scaling performance of cold-rolled enamel steel for water heater liner |
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| CN110095523B (en) * | 2018-01-29 | 2021-05-14 | 宝山钢铁股份有限公司 | Method for predicting scale explosion occurrence probability of enamel product |
| CN111693426A (en) * | 2019-03-15 | 2020-09-22 | 宝山钢铁股份有限公司 | Device and method for evaluating fish scaling performance of enamel steel |
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